United States Patent (19) 11 Patent Number: 4,461,660

Binet et al. 45) Date of Patent: Jul. 24, 1984

54) BULK MANUFACTURE OF EMULSION 56) References Cited
EXPLOSIVES U.S. PATENT DOCUMENTS
3,424,438 M1969 Knotts et al. ................... 86/20 CX
75 Inventors: Rejean Binet, St. Bruno; William E. 4,287,010 9/1981 Owen ............................... 149/109.6
Cribb, Pointe Claire; Anthony C. F.
Edmonds, Burlington; Melvin A. FOREIGN PATENT DOCUMENTS
McNicol, Otterburn Park, all of 7714394 1/1980 Sweden ................................. 366/57
Canada 1284375 8/1972 United Kingdom .................. 366/57
Primary Examiner-Leland A. Sebastian
73 Assignee: C--L Inc., North York, Canada Attorney, Agent, or Firm-Donald G. Ballantyne
57 ABSTRACT
21 Appl. No.: 502,297
A method and apparatus is provided for the efficient
and safe manufacture of batch quantities of non-cap-sen
22 Filed: Jun. 8, 1983 sitive emulsion explosives. The method employs none
of the high shear mixing or homogenizing techniques of
30 Foreign Application Priority Data the prior art and hence hazards from heat and mechani
Jun. 21, 1982 CA) Canada ................................... 405639
cal breakdown (impact) are eliminated. The method
consists of tumbling the oil phase of the emulsion in a
rotating, internally baffled mixer and slowly adding
51) Int. Cl. .............................................. CO6B 45/00 thereto the aqueous phase. The resulting emulsion ex
52 U.S. C. ......................................... 149/2; 86/1 R; plosive is detonable by boostering in large diameter
86/20 C, 149/46; 149/109.6; 366/57 charges.
58 Field of Search ................... 86/1 R, 20 C, 149/2,
149/46, 109.6; 366/57, 58, 59,225 8 Claims, 2 Drawing Figures

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U.S. Patent Jul. 24, 1984 4,461,660

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 4,461,660 2
and, thirdly, safety. The monetary or investment con
BULK MANUFACTURE OF EMULSION siderations are self-evident. Where the objective is to
EXPLOSIVES produce a very small droplet size and, hence, sensitive
emulsion explosive designed for blasting cap initiation, a
The present invention relates to a method and appara 5 very high shear mixing apparatus will generally be the
tus for the manufacture of batch or bulk quantities of apparatus of choice. However, use of high shear mixing
non-cap-sensitive water-in-oil emulsion explosives. In apparatus for explosive compositions carries an accom
particular, the invention relates to the batch production panying hazard because of risk of mechanical failure
of relatively insensitive emulsion explosives employing and impact and the generation of heat. Capital invest
a mixing zone containing a substantially shearless mixer. 10 ment is also often high. Where non-cap-sensitive emul
By non-cap-sensitive emulsion explosives is meant a sion explosives are to be manufactured, a medium or
composition which is insensitive to initiation by blasting moderate shear mixer is normally chosen which type of
cap and which must be initiated by strong boostering. mixer possesses most of the disadvantages of a high
Water-in-oil emulsion explosives are now well known shear apparatus. If the explosives manufacturing opera
in the explosives art and have been demonstrated to be 15 tion is to be continuous, both medium and high shear
safe, economical and relatively simple to manufacture mixers can be generally employed for such purposes.
and to yield excellent blasting results. Bluhm, in U.S. The use of in-line motionless mixers may also be conve
Pat. No. 3,447,978, disclosed an emulsion explosive niently adapted for continuous manufacture. Where
composition comprising an aqueous discontinuous manufacture of emulsion explosive is batch-wise, similar
phase containing dissolved oxygen-supplying salts, a 20 high or medium shear mixers either alone or in combi
carbonaceous fuel continuous phase, an occluded gas nation with homogenizers, such as a colloid mill, has
and an emulsifier. Since Bluhm, further disclosures have been deemed essential in order to provide a composition
described improvements and variations in water-in-oil having a uniform distribution of fine droplets. Without
explosives compositions. These include U.S. Pat. No. such a character, the compositions generally lack utility
3,674,578, Cattermole et al.; U.S. Pat. No. 3,770,522, 25 as explosives.
Tomic; U.S. Pat. No. 3,715,247, Wade; U.S. Pat. No. Non-cap-sensitive explosive emulsions which are
3,675,964, Wade; U.S. Pat. No. 4,110,134, Wade; U.S. normally destined for use in the form of large diameter
Pat. No. 4,149,916, Wade; U.S. Pat. No. 4,141,917, packages or borehole charges (7 cm. diameter or
Wade; U.S. Pat. No. 4,141,767, Sudweeks & Jessup; greater), are most conveniently manufactured in batch
Canadian Pat. No. 1,096,173, Binet & Seto; U.S. Pat. 30 quantities. By employing batch manufacture, as op
No. 4,111,727, Clay; U.S. Pat. No. 4,104,092, Mullay; posed to continuous manufacture, the careful propor
U.S. Pat. No. 4,231,821, Sudweeks & Lawrence; U.S. tioned metering of the oil/fuel phase and the aqueous/-
Pat. No. 4,218,272, Brockihgton; U.S. Pat. No. salt phase is avoided and the quality of the finished
4,138,281, Olney & Wade and U.S. Pat. No. 4,216,040, product is, therefore, more easily maintained. In partic
Sudweeks & Jessup. 35 ular, phase inversion is more readily avoided in batch
Emulsion explosive compositions have been manu processing. Nevertheless, it has been the practice in
factured in commercial quantities by means of both batch emulsion explosive manufacture to employ the
batch and continuous processes employing conven same high shear or relatively high shear mixers as are
tional high shear mixing apparatus. Generally, the prior used in continuous manufacture in order to achieve the
art has not been specific in suggesting any particular desired product homogeneity heretofore noted. Conse
mixing or emulsifying apparatus or techniques, refer quently, the problems associated with the use of rapidly
ences usually being made merely to "agitation' or "mix rotating mixing devices, namely, heat generation, me
ing' or "blending' of the aqueous phase and the oil chanical breakdown and high capital and operating
phase in the presence of an emulsifier. Cattermole et al, costs, persist.
in U.S. Pat. No. Re. 28060, refer to the use of a turbine 45 It has now been found that high quality, stable, non
mixer. Chrisp, in U.S. Pat. No. 4,008,108, refers to a cap-sensitive explosive emulsion can be prepared in
high shear mixer, that is, a shear pump. Olney, in U.S. batch quantities without the use of any high shear mix
Pat. No. 4,138,281, suggests the possible use of a contin ing apparatus. It has also been found that the method
uous recycle mixer, for example, the VOTATOR (Reg and apparatus of the invention as hereinafter described
TM) mixer, an in-line mixer, for example, the TURBON 50 may be employed either at a fixed (factory) location or
(Reg TM) and a colloid type mixer, for example, the may be employed mounted upon a mobile carrier for
OAKES (Reg TM). In recent Canadian Pat. No. manufacture of the explosives directly at the blasting
1,106,835, Aanonsen et al describe the use of a mixing site. Furthermore, the method and apparatus of the
unit comprising a turbine-shaped mixing rotor or impel invention permit the production of a stable, very high
ler encased in a housing. In co-pending Canadian Appli 55 phase ratio water-in-oil emulsion (up to 95% water
cation No. 395,372 use is made of a recirculation loop phase) without phase inversion.
containing a pump and an in-line motionless mixer for The method of the invention comprises the steps of
the continuous production of explosive emulsion pre introducing a measured quantity of an oil/surfactant
cursors. In U.S. Pat. No. 4,287,010, J. H. Owen makes phase into an internally baffled, substantially cylindri
use of a blade mixer having a blade tip speed of up to 60 cal, reversibly rotatable drum mixer having an internal
600 cm/sec. In U.S. Pat. No. 4,231,821, Sudweeks et all diameter of at least 1.5 meter and preferably 1.5 to 2.5
employ a colloid mill for the production of small drop meter, and rotating said drum mixer about its longitudi
let emulsions of improved rheology. nal axis at between 8-16 revolutions per minute, while
The choice of an appropriate mixer for the manufac adding thereto a measured quantity of an aqueous
ture of emulsion explosive compositions will depend, in 65 phase, the said aqueous phase addition being made con
large part, upon three principal considerations; firstly, tinuously over a period of not less than 10 minutes to
the desired sensitivity of the final product; secondly, the permit a free fall of material within the drum at a drop
type of operation, whether batch-wise or continuous; velocity of 5 to 7 meter/second to produce an emulsi
 4,461,660
3 4.
fied explosive having a droplet size distribution of from
1-10 um.
The batch mixer apparatus of the invention consists
of a substantially cylindrical shell having a longitudinal
axis, a closed end and an open end for receiving material
to be mixed and for discharging mixed material, said
shell being reversibly rotatable about said axis, and a
plurality of spaced-apart, projecting inclined baffles
positioned on an inner wall of said shell, said baffles
being disposed generally transversely of the said shell
axis, the said baffles being positioned so that upon
clockwise rotation of said shell, flowable material
within said shell is moved towards the said closed shell
end and upon counterclockwise rotation, material is
moved towards and through the said open shell end, the
said projecting portion of said baffles providing a means
to lift material within said shell to the apex of shell
rotation and to release said material to fall by gravity to
the base of said shell.
To provide a better understanding of the invention,
reference is made to the accompanying drawing
wherein:
FIG. 1 shows a perspective view, partly broken
away, of the mixer apparatus of the invention; and
FIG. 2 shows a diagrammatic or schematic represen 25
tation of the process of the invention.
Referring to the drawings, the explosive emulsion
mixer apparatus of the invention which is generally
indicated by reference numeral 1, includes a hollow, 30
generally cylindrical rotatable housing or shell 2 prefer
ably of welded metal construction, having an open end
3 and a closed end 4. Fixed, preferably by welding, to
the mixer inner walls of shell 2 are a series of diagonally
disposed blades or flights 5 which are arranged to direct 35
flowable material within shell 2 towards closed end 4
when shell 2 is in clockwise rotation. Flights 5c and 5d
are more particularly arranged to mainly elevate flow
able material during rotation and, at the apex, to allow
the flowable material to drop away and fall to the base
of shell 2.
Referring particularly to FIG. 2, a hopper 6 is shown
adjacent to open end 3 of shell 2. Passing through
hopper 6 and into opening 3 are delivery conduits, as
shown, for the various components of the emulsion
explosive composition. The lower portion 6a of hopper
6 acts as a collector for the emulsified composition after
mixing has been completed. A pump 7 is conveniently
provided to withdraw the mixed emulsions from hopper
6a after which the emulsion is passed through hose 8
mounted on hose reel 9. An additive reservoir 10 con
taining, for example, a gassing agent is located for deliv
ery of its product to the emulsion at a point close to
pump 7. Alternatively, the mixed emulsion may be
withdrawn from hopper 6a by gravity methods. 55
The emulsification of aqueous and oil phases within
shell 2 is achieved by low speed rotation of the shell,
rotation being accomplished, for example, by means of
a hydraulic motor (not shown) or other known meth
ods. After the placing of the components of the emul 60
sion composition in the shell, as hereinafter described,
the shell is rotated at slow speed, for example, about
8-16 rmp., for a period sufficiently long to produce a
water-in-oil emulsion of desired droplet size. After the
mixing period, the direction of rotation of shell 2 is 65
reversed and the internal flights 5 move the emulsified
composition through opening 3 and into hopper 6a from
where it is removed either by pumping or gravity.
In the operation of the method and apparatus of the
invention, a premeasured or preweighed oil phase is
first introduced into shell 2 and slow clockwise rotation,
about 10 rpm., of shell 2 is begun. The premeasured
aqueous phase is then gradually added to the oil phase
over a period of from 10–60 minutes depending onthe
size of the latch being prepared. It has been found that
if the addition of the aqueous phase is hurried, for exam
ple, in less than 10 minutes, the required small droplet
10 size required in the final product may not be achieved.
The combination of slow addition and long residual
time in a low shear mixing apparatus produces an emul
sion explosive composition having a droplet size distri
bution of about 1-10 um with an average about 4 um.
5 Such a droplet size distribution provides an explosive
product of excellent stability and rheology yet one
which is insensitive to initiation by electric blasting cap.
After mixing to the desired droplet size distribution,
particulate solids or dopes, for example, particulate
20 oxygen-supplying salts, such as prilled ammonium ni
trate or particulate light metal may be added to shell 2
and incorporated into the emulsion. The direction of
rotation of shell 2 is thereafter reversed and the contents
delivered through opening 3 and deposited in hopper
6a,
EXAMPLE I
300 kilograms of a hot (60° C) oil phase was placed
into a 7.6 cubic meter capacity mixing shell. The oil
phase consisted of 45 part paraffin oil, 26 part paraffin
wax and 20 part emulsifier. The shell was rotated in
clockwise rotation at 10 rpm. while 3307 kilograms of a
hot (70° C.) aqueous salt solution phase was added over
a period of 20 minutes. The aqueous phase consisted of
15.35% by weight of water, 61.63% ammonium nitrate,
19.75% sodium nitrate and 0.27% zinc nitrate. After
addition of the aqueous phase was completed, the re
sulting emulsion was mixed at 10 rpm. for a further 10
minutes. The rotation rate was then reduced to 2 rpm.
and 907 kilograms of particulate ammonium nitrate was
added and blended into the emulsion. Rotation of the
mixing shell was reversed and the mixed composition
collected in a hopper from which it was packaged into
plastic bag-like containers with the addition of sodium
45 nitrite to generate some nitrogen bubbles. The composi
tion was insensitive to initiation by electric blasting cap
and had a density of 1.10. Upon detonation by means of
a 60 gram pentolite booster in 16.5 cm. diameter
charges, the composition had a velocity of detonation of
50 4800 m.p.s., which value was unchanged after 3 weeks
storage at 5 C.
It will be appreciated by those skilled in the art that
the non-cap-sensitive product heretofore described may
be rendered sensitive to cap initiation by the incorpora
tion of density lowering ingredients, such as further gas
bubbles, glass or resin micropheres, verniculite and the
like, or by the incorporation of self-explosives such as,
for example, particulate TNT.
EXAMPLE II
193 kilograms of a hot (60° C) oil phase was placed
into a 7.6 cubic meter capacity mixing shell. This oil
phase consisted of 28 parts emulsifier, 41 parts paraffin
oil and 31 parts paraffin wax. As in Example I, 3003
kilograms of a hot aqueous phase with the same compo
sition as Example I was added over 25 minutes with the
mixer rotating at 12 rpm. After addition of the aqueous
phase was completed, the resulting emulsion was mixed
 4,461,660
5 6
at 10 rpm for 10 minutes. The rotation rate was then
reduced to 2 rpm and 750 kilograms of particulate TNT
was added and blended into the emulsion. The product
was discharged as for Example I directly into bore
holes, except that no gassing agent was added. The
density was 1.50. The product was kept for 3 weeks and
upon detonation by means of a 450 g pentolite/TNT
booster in 20 cm. diameter boreholes had a velocity of
detonation of 4.8 km sl. A similar product in 12.7 cm.
diameter packages shoots when initiated with 230 g of
pentolite.
EXAMPLE III
An emulsion explosive was made as for Example I
except that 308 kilograms of an oil phase containing
22% surfactant, 45% paraffin oil and 33% wax was
used. To this was added 4205 kilograms of an
AN/SN/ZN/H2O liquor as for Example I. The prod
uct was mixed and discharged directly to a borehole
with addition of NaNO2 to produce gassing and lower
the density to 1.10 g/cc. Upon detonation with a 450 g
booster the product had a velocity of detonation of 5.5
km s in 20 cm. diameter boreholes.
It is postulated that the surprising and unexpected 25
production of very small droplet emulsion explosives by
employing a baffled, rotating shell, batch mixer is due to
a combination of turbulence and vortexing which oc
curs during mixing. The rotation of the shell causes the
fluid contents to flow over the baffles or flights and to 30
fall by gravity to the pool of material below. Such flow
and splashing and the turbulence resulting therefrom
cause vortices and whirlpools of a range of sizes which
results in the production of droplets of a corresponding
range of sizes. 35
Where the mixer apparatus of the invention is
mounted at a fixed location, the various liquid compo
nents or phases of the emulsion explosives composition
can be prepared in separate heated mixers of conven
tional construction, e.g., paddle mixers. These phases
can then be added to the emulsion mixer in preweighed
or premeasured quantities as hereinbefore described.
Similarly, any solid ingredients or dopes can be added
from, for example, volumetric storage bins or weigh 45
hoppers.
Where on-site mixing is performed, the mixer appara
tus of the invention can be mounted upon a vehicle or a
vehicle-pulled trailer. The liquid phases and solid addi
tives can be carried in premeasured amounts in insulated 50
and/or heated storage containers mounted upon the
vehicle or trailer or carried on a separate nurse vehicle.
After the emulsion has been prepared in a batch quan
tity, the mixer vehicle can move from borehole to bore
hole until all holes are filled or until the supply of mixed
explosives is exhausted.
We claim:
1. A method of manufacture of a high phase ratio
water-in-oil emulsion explosive composition which is
insensitive to blasting cap initiation comprising the steps
of:
(a) introducing a measured quantity of an oil/surfact
ant phase into an internally baffled, substantially
5 cylindrical, reversibly rotatable drum mixer having
an internal diameter of at least 1.5 meter and prefer
ably 1.5 to 2.5 meter,
(b) rotating said drum mixer about its longitudinal
axis at between 8-16 revolutions per minute, while
10 adding thereto a measured quantity of an aqueous
phase, the said aqueous phase addition being made
continuously over a period of not less than 10 min
utes to permit a free fall of material within the
drum at a drop velocity of 5 to 7 meter/second to
15 produce an emulsified explosive having a droplet
size distribution of from 1-10 um,
2. A method as claimed in claim 1 also comprising the
step of adding to the said emulsified explosive measured
quantities of particulate solid materials.
3. A method as claimed in claim 1 also comprising the
step of incorporating into said emulsifier explosive a
density reducing agent.
4. A method as claimed in claim 2 wherein the said
particulate solid material is selected from oxygen sup
plying salts, light metals and self explosives.
5. A method as claimed in claim 3 wherein the said
density reducing agent comprises gas bubbles, void
containing particulate material or mixtures of these.
6. A batch mixer for the manufacture of non-cap-sen
sitive water-in-oil emulsion explosives comprising:
(a) a substantially cylindrical shell having alongitudi
nal axis, a closed end and an open end for receiving
material to be mixed and for discharging mixed
material, said shell having an internal diameter of at
least 1.5 meter and preferably 1.5 to 2.5 meter being
reversibly rotatable about said axis, and
(b) a plurality of spaced-apart, projecting inclined
baffles positioned on an inner wall of said shell, said
baffles being disposed generally transversely of the
said shell axis, the said baffles being positioned so
that upon clockwise rotation of said shell, flowable
material within said shell is moved towards the said
closed shell end and upon counterclockwise rota
tion, material is moved towards and through the
said open shell end, the said projecting portion of
said baffles providing a means to lift material
within said shell to the apex of shell rotation and to
release said material to fall by gravity to the base of
said shell at a drop velocity of from 5 to 7 meter/-
second.
7. A mixer apparatus as claimed in claim 6 also com
prising a receiver means adjacent the said shell open end
for collection therein of mixed emulsion explosive
moved through the said shell open end, said receiver
55 means having directional means on the base thereof for
delivering said collected emulsion to a selected locality.
8. A mixer as claimed in claim 6 wherein the drum
internal diameter is 1.5 to 2.5 meter.
s sk s g
60
65